# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Daofeng Sun' _publ_contact_author_email dfsun@sdu.edu.cn _publ_author_name 'Daofeng Sun' data_squeezed1 _database_code_depnum_ccdc_archive 'CCDC 831821' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H13.75 N O7 Zn2' _chemical_formula_weight 690.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.854(6) _cell_length_b 17.042(4) _cell_length_c 20.656(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.017(4) _cell_angle_gamma 90.00 _cell_volume 8812(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2774 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8959 _exptl_absorpt_correction_T_max 0.9155 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14611 _diffrn_reflns_av_R_equivalents 0.0851 _diffrn_reflns_av_sigmaI/netI 0.1044 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 20.89 _reflns_number_total 4621 _reflns_number_gt 2260 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4621 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1271 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2286 _refine_ls_wR_factor_gt 0.2064 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.883 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.0917(4) 0.0585(5) -0.0653(5) 0.070(2) Uani 1 1 d . . . Zn1 Zn 0.13893(5) 0.06800(7) 0.04076(6) 0.0638(5) Uani 1 1 d . . . Zn2 Zn 0.20059(5) 0.06933(7) 0.22453(7) 0.0720(5) Uani 1 1 d . . . O1 O 0.1556(4) -0.0270(4) 0.1861(5) 0.097(3) Uani 1 1 d . . . O2 O 0.1113(3) -0.0217(4) 0.0691(5) 0.090(3) Uani 1 1 d . . . O3 O -0.2535(3) -0.4297(5) 0.1718(5) 0.103(3) Uani 1 1 d . . . O4 O -0.2899(4) -0.4448(5) 0.0547(5) 0.096(3) Uani 1 1 d . . . O5 O 0.1539(4) -0.8389(5) 0.1829(6) 0.123(4) Uani 1 1 d . . . O6 O 0.1199(3) -0.8338(4) 0.0649(5) 0.092(3) Uani 1 1 d . . . O8 O 0.2225(13) 0.0593(10) 0.3280(9) 0.46(2) Uani 1 1 d . . . C1 C 0.1266(5) -0.0556(7) 0.1282(7) 0.070(3) Uani 1 1 d . . . C2 C 0.1046(4) -0.1353(6) 0.1291(7) 0.056(3) Uani 1 1 d . . . C3 C 0.1181(4) -0.1742(6) 0.1907(6) 0.071(3) Uani 1 1 d . . . H3 H 0.1427 -0.1528 0.2340 0.085 Uiso 1 1 calc R . . C4 C 0.0953(4) -0.2467(6) 0.1895(6) 0.070(3) Uani 1 1 d . . . H4 H 0.1046 -0.2732 0.2327 0.084 Uiso 1 1 calc R . . C5 C 0.0597(4) -0.2805(5) 0.1270(6) 0.050(3) Uani 1 1 d . . . C6 C 0.0472(4) -0.2423(6) 0.0638(6) 0.073(3) Uani 1 1 d . . . H6 H 0.0245 -0.2647 0.0200 0.088 Uiso 1 1 calc R . . C7 C 0.0693(5) -0.1693(7) 0.0668(7) 0.078(3) Uani 1 1 d . . . H7 H 0.0596 -0.1418 0.0240 0.094 Uiso 1 1 calc R . . C8 C 0.0336(4) -0.3617(6) 0.1263(5) 0.052(3) Uani 1 1 d . . . C9 C 0.0587(4) -0.4317(6) 0.1213(5) 0.049(2) Uani 1 1 d . . . C10 C 0.1119(4) -0.4277(5) 0.1159(6) 0.070(3) Uani 1 1 d . . . H10A H 0.1216 -0.3738 0.1150 0.104 Uiso 1 1 calc R . . H10B H 0.1081 -0.4533 0.0726 0.104 Uiso 1 1 calc R . . H10C H 0.1392 -0.4534 0.1569 0.104 Uiso 1 1 calc R . . C11 C 0.0357(4) -0.5013(6) 0.1235(5) 0.044(2) Uani 1 1 d . . . C12 C -0.0125(5) -0.5048(5) 0.1257(5) 0.057(3) Uani 1 1 d . . . C13 C -0.0397(4) -0.4352(6) 0.1270(5) 0.050(2) Uani 1 1 d . . . C14 C -0.0149(4) -0.3636(6) 0.1307(5) 0.055(3) Uani 1 1 d . . . C15 C -0.0413(4) -0.2851(5) 0.1373(5) 0.060(3) Uani 1 1 d . . . H15A H -0.0185 -0.2419 0.1393 0.090 Uiso 1 1 calc R . . H15B H -0.0462 -0.2859 0.1804 0.090 Uiso 1 1 calc R . . H15C H -0.0753 -0.2791 0.0962 0.090 Uiso 1 1 calc R . . C16 C 0.0633(4) -0.5753(6) 0.1236(6) 0.059(3) Uani 1 1 d . . . C17 C 0.0614(4) -0.6083(7) 0.0642(6) 0.066(3) Uani 1 1 d . . . H17 H 0.0435 -0.5812 0.0210 0.079 Uiso 1 1 calc R . . C18 C 0.0839(4) -0.6792(7) 0.0617(6) 0.073(3) Uani 1 1 d . . . H18 H 0.0833 -0.6976 0.0189 0.087 Uiso 1 1 calc R . . C19 C 0.1077(4) -0.7229(6) 0.1247(7) 0.068(3) Uani 1 1 d . . . C20 C 0.1125(5) -0.6916(7) 0.1903(6) 0.091(4) Uani 1 1 d . . . H20 H 0.1306 -0.7184 0.2335 0.109 Uiso 1 1 calc R . . C21 C 0.0890(5) -0.6193(8) 0.1878(6) 0.094(4) Uani 1 1 d . . . H21 H 0.0903 -0.5987 0.2303 0.113 Uiso 1 1 calc R . . C23 C -0.0933(4) -0.4373(5) 0.1254(5) 0.053(3) Uani 1 1 d . . . C24 C -0.0995(4) -0.4342(5) 0.1876(6) 0.064(3) Uani 1 1 d . . . H24 H -0.0697 -0.4320 0.2321 0.077 Uiso 1 1 calc R . . C25 C -0.1508(5) -0.4344(6) 0.1841(6) 0.071(3) Uani 1 1 d . . . H25 H -0.1546 -0.4311 0.2265 0.086 Uiso 1 1 calc R . . C26 C -0.1960(5) -0.4395(5) 0.1189(6) 0.062(3) Uani 1 1 d . . . C27 C -0.1894(4) -0.4434(6) 0.0567(6) 0.081(3) Uani 1 1 d . . . H27 H -0.2192 -0.4469 0.0123 0.098 Uiso 1 1 calc R . . C28 C -0.1383(5) -0.4419(6) 0.0599(6) 0.085(4) Uani 1 1 d . . . H28 H -0.1343 -0.4441 0.0175 0.103 Uiso 1 1 calc R . . C30 C -0.2516(5) -0.4379(6) 0.1138(8) 0.069(3) Uani 1 1 d . . . C31 C -0.0430(5) -0.5803(5) 0.1216(7) 0.083(4) Uani 1 1 d . . . H31A H -0.0757 -0.5680 0.1244 0.125 Uiso 1 1 calc R . . H31B H -0.0216 -0.6140 0.1609 0.125 Uiso 1 1 calc R . . H31C H -0.0511 -0.6064 0.0768 0.125 Uiso 1 1 calc R . . C32 C 0.1277(5) -0.8058(8) 0.1240(8) 0.077(4) Uani 1 1 d . . . C33 C 0.1064(5) 0.0614(9) -0.1151(7) 0.116(5) Uani 1 1 d . . . H33 H 0.1429 0.0654 -0.1012 0.139 Uiso 1 1 calc R . . C34 C 0.0734(6) 0.0590(9) -0.1880(7) 0.131(6) Uani 1 1 d . . . H34 H 0.0876 0.0598 -0.2212 0.157 Uiso 1 1 calc R . . C35 C 0.0197(5) 0.0554(6) -0.2105(5) 0.071(3) Uani 1 1 d . . . C36 C 0.0023(6) 0.0536(8) -0.1592(7) 0.109(5) Uani 1 1 d . . . H36 H -0.0342 0.0509 -0.1721 0.130 Uiso 1 1 calc R . . C37 C 0.0380(6) 0.0558(8) -0.0881(7) 0.112(5) Uani 1 1 d . . . H37 H 0.0250 0.0554 -0.0537 0.134 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.066(7) 0.080(6) 0.064(6) -0.012(5) 0.028(6) -0.007(5) Zn1 0.0601(9) 0.0611(9) 0.0623(9) -0.0015(7) 0.0195(7) 0.0025(7) Zn2 0.0707(10) 0.0704(10) 0.0751(10) 0.0040(8) 0.0320(8) -0.0007(7) O1 0.107(7) 0.069(6) 0.091(7) -0.001(5) 0.021(6) -0.028(5) O2 0.088(6) 0.078(6) 0.088(6) 0.006(5) 0.023(5) -0.038(5) O3 0.084(7) 0.115(7) 0.133(8) 0.007(6) 0.068(6) -0.003(5) O4 0.066(6) 0.125(7) 0.094(7) -0.014(6) 0.033(5) -0.018(5) O5 0.190(11) 0.067(6) 0.136(9) 0.025(6) 0.094(8) 0.056(6) O6 0.082(6) 0.077(6) 0.101(7) -0.013(5) 0.025(5) 0.016(4) O8 0.82(6) 0.24(2) 0.153(14) -0.070(13) 0.06(2) -0.20(2) C1 0.085(10) 0.059(9) 0.051(8) 0.000(7) 0.016(7) 0.003(7) C2 0.041(7) 0.039(7) 0.075(9) 0.017(7) 0.014(6) 0.003(5) C3 0.059(8) 0.047(7) 0.085(9) 0.002(7) 0.012(7) -0.020(6) C4 0.065(9) 0.068(8) 0.069(8) -0.003(7) 0.022(7) -0.002(7) C5 0.046(7) 0.033(6) 0.069(8) 0.000(6) 0.023(6) -0.007(5) C6 0.067(8) 0.059(8) 0.078(9) 0.013(7) 0.018(7) -0.020(6) C7 0.082(10) 0.062(8) 0.081(9) 0.021(7) 0.027(8) 0.001(7) C8 0.047(7) 0.058(7) 0.051(7) -0.009(5) 0.020(6) -0.016(6) C9 0.044(6) 0.054(7) 0.056(6) -0.002(6) 0.028(5) 0.004(6) C10 0.071(8) 0.063(7) 0.082(8) 0.006(6) 0.040(7) 0.018(6) C11 0.024(6) 0.045(7) 0.065(7) 0.003(5) 0.021(5) 0.003(5) C12 0.084(9) 0.026(6) 0.060(7) 0.003(5) 0.029(7) -0.001(6) C13 0.041(6) 0.057(7) 0.052(6) -0.008(5) 0.021(5) -0.009(6) C14 0.053(8) 0.070(8) 0.046(6) 0.000(5) 0.024(6) -0.007(6) C15 0.051(7) 0.064(7) 0.064(7) 0.005(5) 0.023(6) 0.010(5) C16 0.059(8) 0.057(8) 0.060(7) 0.004(7) 0.024(6) -0.011(6) C17 0.075(9) 0.076(9) 0.046(7) 0.004(6) 0.027(6) 0.005(7) C18 0.071(9) 0.076(9) 0.062(8) 0.002(7) 0.022(7) 0.019(7) C19 0.049(7) 0.057(8) 0.105(11) -0.017(8) 0.040(7) 0.013(6) C20 0.144(12) 0.073(9) 0.053(8) 0.007(7) 0.040(8) 0.039(8) C21 0.124(12) 0.087(10) 0.063(9) -0.016(8) 0.033(8) 0.028(9) C23 0.061(8) 0.048(6) 0.053(7) -0.009(6) 0.027(6) -0.002(6) C24 0.042(7) 0.076(8) 0.073(8) -0.004(7) 0.025(6) -0.001(6) C25 0.079(9) 0.084(8) 0.064(8) -0.001(7) 0.042(8) -0.009(7) C26 0.069(9) 0.057(7) 0.078(8) -0.007(7) 0.047(8) -0.009(6) C27 0.037(8) 0.123(10) 0.064(8) -0.018(7) 0.004(6) 0.009(7) C28 0.064(9) 0.118(10) 0.072(9) -0.019(8) 0.027(7) -0.015(8) C30 0.083(11) 0.053(7) 0.090(10) 0.002(8) 0.057(9) -0.005(7) C31 0.098(10) 0.045(7) 0.124(10) 0.002(6) 0.065(8) 0.007(6) C32 0.054(8) 0.091(11) 0.089(11) 0.022(9) 0.033(8) 0.018(7) C33 0.057(9) 0.225(17) 0.073(10) -0.016(11) 0.034(8) -0.056(10) C34 0.058(10) 0.260(19) 0.069(10) -0.003(11) 0.022(8) -0.048(11) C35 0.086(11) 0.066(8) 0.059(7) 0.012(5) 0.029(7) 0.004(6) C36 0.085(11) 0.169(14) 0.078(10) 0.006(10) 0.041(9) 0.036(9) C37 0.064(11) 0.208(16) 0.062(9) 0.011(10) 0.027(8) 0.035(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C33 1.264(13) . ? N1 C37 1.357(14) . ? N1 Zn1 2.008(9) . ? Zn1 O4 1.885(9) 3 ? Zn1 O6 1.887(8) 1_565 ? Zn1 O2 1.914(7) . ? Zn2 O8 1.956(17) . ? Zn2 O5 1.973(9) 1_565 ? Zn2 O1 2.005(8) . ? Zn2 O3 2.012(9) 3 ? O1 C1 1.213(11) . ? O2 C1 1.246(11) . ? O3 C30 1.230(12) . ? O3 Zn2 2.012(9) 3_445 ? O4 C30 1.225(13) . ? O4 Zn1 1.885(9) 3_445 ? O5 C32 1.246(13) . ? O5 Zn2 1.973(9) 1_545 ? O6 C32 1.239(13) . ? O6 Zn1 1.887(8) 1_545 ? C1 C2 1.494(15) . ? C2 C3 1.333(12) . ? C2 C7 1.359(13) . ? C3 C4 1.386(13) . ? C3 H3 0.9300 . ? C4 C5 1.363(12) . ? C4 H4 0.9300 . ? C5 C6 1.362(12) . ? C5 C8 1.559(12) . ? C6 C7 1.377(13) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C14 1.391(12) . ? C8 C9 1.409(12) . ? C9 C11 1.358(11) . ? C9 C10 1.535(12) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.366(12) . ? C11 C16 1.475(13) . ? C12 C13 1.413(12) . ? C12 C31 1.522(12) . ? C13 C14 1.388(12) . ? C13 C23 1.481(13) . ? C14 C15 1.562(12) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.330(12) . ? C16 C21 1.415(14) . ? C17 C18 1.374(13) . ? C17 H17 0.9300 . ? C18 C19 1.389(13) . ? C18 H18 0.9300 . ? C19 C20 1.406(13) . ? C19 C32 1.521(15) . ? C20 C21 1.386(14) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C23 C24 1.371(12) . ? C23 C28 1.385(14) . ? C24 C25 1.396(14) . ? C24 H24 0.9300 . ? C25 C26 1.386(14) . ? C25 H25 0.9300 . ? C26 C27 1.376(13) . ? C26 C30 1.504(15) . ? C27 C28 1.398(15) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C33 C34 1.379(16) . ? C33 H33 0.9300 . ? C34 C35 1.357(16) . ? C34 H34 0.9300 . ? C35 C36 1.348(15) . ? C35 C35 1.51(2) 2_554 ? C36 C37 1.365(16) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C33 N1 C37 114.9(10) . . ? C33 N1 Zn1 126.4(9) . . ? C37 N1 Zn1 118.5(8) . . ? O4 Zn1 O6 117.4(4) 3 1_565 ? O4 Zn1 O2 113.4(4) 3 . ? O6 Zn1 O2 115.5(4) 1_565 . ? O4 Zn1 N1 107.4(4) 3 . ? O6 Zn1 N1 103.6(4) 1_565 . ? O2 Zn1 N1 96.3(4) . . ? O8 Zn2 O5 112.1(9) . 1_565 ? O8 Zn2 O1 101.7(6) . . ? O5 Zn2 O1 107.4(4) 1_565 . ? O8 Zn2 O3 128.7(11) . 3 ? O5 Zn2 O3 102.2(4) 1_565 3 ? O1 Zn2 O3 103.1(4) . 3 ? C1 O1 Zn2 138.5(9) . . ? C1 O2 Zn1 131.3(8) . . ? C30 O3 Zn2 146.7(9) . 3_445 ? C30 O4 Zn1 122.7(8) . 3_445 ? C32 O5 Zn2 141.0(9) . 1_545 ? C32 O6 Zn1 130.9(9) . 1_545 ? O1 C1 O2 125.0(12) . . ? O1 C1 C2 116.9(11) . . ? O2 C1 C2 117.9(11) . . ? C3 C2 C7 118.4(10) . . ? C3 C2 C1 121.2(11) . . ? C7 C2 C1 120.4(11) . . ? C2 C3 C4 119.4(11) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 122.1(10) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C6 C5 C4 118.6(9) . . ? C6 C5 C8 119.7(9) . . ? C4 C5 C8 121.8(10) . . ? C5 C6 C7 118.0(11) . . ? C5 C6 H6 121.0 . . ? C7 C6 H6 121.0 . . ? C2 C7 C6 123.3(11) . . ? C2 C7 H7 118.3 . . ? C6 C7 H7 118.3 . . ? C14 C8 C9 120.7(8) . . ? C14 C8 C5 118.8(9) . . ? C9 C8 C5 120.5(9) . . ? C11 C9 C8 118.8(8) . . ? C11 C9 C10 121.6(9) . . ? C8 C9 C10 119.6(9) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C12 121.6(8) . . ? C9 C11 C16 119.7(9) . . ? C12 C11 C16 118.7(9) . . ? C11 C12 C13 120.4(8) . . ? C11 C12 C31 124.6(9) . . ? C13 C12 C31 114.8(10) . . ? C14 C13 C12 118.8(9) . . ? C14 C13 C23 119.7(9) . . ? C12 C13 C23 121.5(9) . . ? C13 C14 C8 119.4(9) . . ? C13 C14 C15 121.0(9) . . ? C8 C14 C15 119.5(9) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 116.1(10) . . ? C17 C16 C11 123.3(10) . . ? C21 C16 C11 120.3(10) . . ? C16 C17 C18 124.9(11) . . ? C16 C17 H17 117.5 . . ? C18 C17 H17 117.5 . . ? C17 C18 C19 118.3(10) . . ? C17 C18 H18 120.9 . . ? C19 C18 H18 120.9 . . ? C18 C19 C20 120.3(10) . . ? C18 C19 C32 121.0(11) . . ? C20 C19 C32 118.7(12) . . ? C21 C20 C19 117.3(10) . . ? C21 C20 H20 121.4 . . ? C19 C20 H20 121.4 . . ? C20 C21 C16 122.9(10) . . ? C20 C21 H21 118.6 . . ? C16 C21 H21 118.6 . . ? C24 C23 C28 119.1(10) . . ? C24 C23 C13 121.3(9) . . ? C28 C23 C13 119.6(9) . . ? C23 C24 C25 119.8(10) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 121.6(10) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C27 C26 C25 118.2(10) . . ? C27 C26 C30 119.3(12) . . ? C25 C26 C30 122.4(11) . . ? C26 C27 C28 120.4(10) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C23 C28 C27 120.8(10) . . ? C23 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? O4 C30 O3 126.2(12) . . ? O4 C30 C26 119.3(12) . . ? O3 C30 C26 114.6(13) . . ? C12 C31 H31A 109.5 . . ? C12 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C12 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O6 C32 O5 124.1(13) . . ? O6 C32 C19 117.5(12) . . ? O5 C32 C19 118.2(13) . . ? N1 C33 C34 125.9(12) . . ? N1 C33 H33 117.0 . . ? C34 C33 H33 117.0 . . ? C35 C34 C33 118.9(12) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C36 C35 C34 117.0(11) . . ? C36 C35 C35 120.3(16) . 2_554 ? C34 C35 C35 122.7(14) . 2_554 ? C35 C36 C37 120.0(13) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? N1 C37 C36 123.2(11) . . ? N1 C37 H37 118.4 . . ? C36 C37 H37 118.4 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 20.89 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.945 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.097